Process of obtaining iodine



(NQ Model.) 4 Sheets-Sheet ,1,

11.151. WING. PROGESS 0F OBTAINING IODINE.

110.456,183. Patented Ju1y 21,1891.

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H H WING PRooEss 'or OBTAINING IQDINL No. 456,183. Pafented July 21,1891.

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No. 456,183. Patented'my 21,1891.

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H H WING PROCESS 0F OBTAINING IOYDINE.

' Patented Jul-y 21,1891.

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HERBERT H. VING, OF BUFFALO, NEXV YORK.

PROCESS OF OBTAINING IODINE.

SPECIFICATION forming part of Letters Patent No. 456,183, dated July 21, 1891.

Application led November l, 1890. Serial No. 370,081. (No model.)

To all whom, it may concern-.f-

Be it known that I, HERBERT H. VING, a citizen ofthe United States, residing at the city of Buffalo, in the county of Erie and State of New York, have invented a new and use-f ful Improvement in the Method oi Manufacturing Iodine, of which the following is a specification.

This invention relates to the manufacture of iodine, and has the object to produce iodine in a simple and inexpensive manner.

In the accompanying drawings, consisting of four sheets, Figure l is a sectional elevation of an apparatus by which my invention can be practiced. Fig. 2 is a top plan view thereof. Fig. 3 is a sectional elevation of another construction of apparatus whereby my invention can be practiced., Fig. et is a horizontal section of the furnace in line a: Fig. 3, on an enlarged scale. Fig. 5 is a top plan View of the apparatus represented in Fig. 3. Fig. G is a horizontal section in line y y, Fig.

i l, on an enlarged scale.

Like letters of reference refer to like parts in the several figures.

In practicing my invention I use the motherliquor, called aqua vieja, obtained from the purification of crude ohilisaltpeter, (sodium nitrate.) This mother-liquor contains the iodine,probablyin the form of sodium iodate (NaIO3,) with some sodium iodide (Nal.) This mother-liquor is evaporated to a slrupy consist-ency, and then clay or any other silicious material in a finely-divided state is mixed with it in such proportion as to form aplastic mass, which is molded into balls, .preferably two to three inches in diameter. These balls are dried and then calcin'ed in a suitable fur-x nace or kiln to a semi-fused mass, whereby the iodine is expelled. The fumes of iodine are condensed in subli min g-chambers, and the uncondensed gases and vapors, I consisting largely of the products of combust1on, nitrous acid, chlorine gas, and sulphurous and sulphuric acids in varying proportlons, according to the composition of the mother-liquor, are passed through a furtherl quantity of mother-liqu or. The nitrous ac id, s ulphurous acid, and chlorine gas in coming 1n contact with the mother-liquor precipitate the iodine contained in the same, so that a portion of the m other-liquor is deprived of the iodine by additional portion of mother-liquor is deprived of its iodine by treatment with the waste gases resulting from the calcination. This treatment of mother-liquor with the waste gases maybe omitted, if desired; but I prefer to employ it, as it materially increases the yield of iodine Without materially increasing the expense.

In the apparatus, represented in Figs. l and calcination with a silicious material, and an 2, A represents the kiln or furnace in which 1 the mixture of silicious material and mother-4 liquor is calcined, 'and which is preferably provided with gas-burners a for heating it.

h is the pipe through which the gases and vapors escape from the top of the furnace.

O O represent two subliming-chambers, in

which the iodine is condensed and which are connected with the pipe b by branch pipes d d', provided with cocks c c', so that one of the subliming-chambers can be shut olf for removing the deposited iodine while the other subliming-chamber is in use. Each subliming-chamber has its'top plate covered with a water-jacket f, through which water is circulated by pipes j and which keeps the top plate cool, so that the iodine contained in the vapor is deposited on the under side of the top plate. The. top plate is made in sections, which are hinged to the body of the sublimin g-chamber for ready access to the same.

g g represent branch pipes, which are provided with cocks h h', and by which the vapors and gases pass from the subliming-chain bers to a main pipe H, which leads to the foot of a tower I. The latter is providedv at its top with a sprinkler I, by which mother-liquor is introduced, which is caused to tricklethrough the tower, whilethe vapors and gases ascend through the same and iinall y escape through a waste-pipe i at the top.

The sprinkler may be provided with a number of perforated arms, which are attached to a hub and revolve about the lower end of the supply-pipe, through which the mother-liquor is introduced, as represented in Figs. l and (5, or it may be of any other suitable construction. The tower is illed with coke, broken porcelain, or some other suitable material. The iodine is precipitated in the mother-liquor trickling through the tower by the nitrous acid, sulphurous acid, and chlorine gas con- IOO tained in the vapors and passes with the mother-liquor from the bottom oi the tower through a pipe li; -into settling-tanks K, in which it is deposited and from which it is removed from time to time and further purified.

In the apparatus represented in Figs. 3 and 5 the tower is dispensed with and the Waste gases and vapors pass from each subliiningchamber by a pipe L to a series of washingvessels M, in which the gases and vapors are conducted through mother-liquor, with which the vessels are supplied, in such manner that the mother-liquor enters the Washing-vessel farthest from the subliming chamber and overliows from one vessel into another by pipes fnl and escapes finally from the washing-'vessel nearest the subliming-chamber through an overflow-pipe n. The gases and vapors in passing through the mother-liquor precipitate the iodine, which is removed Jfrom time to time and further purified.

The semi-fused material produced by the calcination consists of silicate of soda, together with silicates of other bases contained in the silieious material and mother-liquor, and this material may be used for obtaining soda, water glass, and other products.

I claim as my inventionl. In the manufacture of iodine, the method oitl producing fumes containing iodine, which consists in mixing silieious material with the mother-'liquor resulting from the purification of sodium nitrate and calciuing the mixture, substantially as set forth.

2. The herein-described method ot' producing iodine, which consists in mixing silieious material With the mother-liquor resulting from the purification of sodium nitrate, calcining the mixture, and collecting the sublimed iodine, substantially as set forth.

3. The herein-described method of producing iodine, which consists in mixing silieious material with the mother-liquor resulting from the purification of sodium nitrate, caleining the mixture, conducting the fumes through a chamber in which the sublimed iodine is collected, and bringing the uncondcnsed vapors in contact with a further quantity of said mother-liquor, whereby a further quantity oi' iodine is precipitated, substantially as set forth.

lVitncss my hand this 28th day of October, 1390.

HERBERT Il. \VING.

lVitnesses:

ARL F. GEYER, Amon G. GONNELLY. 

